U.S. patent application number 16/767587 was filed with the patent office on 2020-12-10 for basic zinc chloride particulate matter and preparation method therefor.
This patent application is currently assigned to GUANGZHOU COSMO ENVIRONMENTAL TECHNOLOGY CO., LTD.. The applicant listed for this patent is GUANGZHOU COSMO ENVIRONMENTAL TECHNOLOGY CO., LTD.. Invention is credited to Zhiyuan HUANG, Hao WANG, Yongcheng WANG, Yangdong WU, Chengwei YE, Zhengjiong ZHA.
Application Number | 20200385282 16/767587 |
Document ID | / |
Family ID | 1000005100669 |
Filed Date | 2020-12-10 |
United States Patent
Application |
20200385282 |
Kind Code |
A1 |
HUANG; Zhiyuan ; et
al. |
December 10, 2020 |
BASIC ZINC CHLORIDE PARTICULATE MATTER AND PREPARATION METHOD
THEREFOR
Abstract
A basic zinc chloride particulate matter and a preparation
method therefor. The basic zinc chloride particulate matter mainly
consists of basic zinc chloride particles. In the basic zinc
chloride particulate matter, D.sub.10>100 .mu.m, and
D.sub.95>450 .mu.m. The basic zinc chloride particles do not
contain adhesives. The basic zinc chloride particles contained in
the basic zinc chloride particulate matter are approximately
spherical, and the basic zinc chloride particles with the particle
diameter >500 .mu.m in the basic zinc chloride particulate
matter accounts for 1% or less of the total mass of the basic zinc
chloride particulate matter.
Inventors: |
HUANG; Zhiyuan; (Guangdong,
CN) ; WU; Yangdong; (Guangdong, CN) ; YE;
Chengwei; (Guangdong, CN) ; WANG; Hao;
(Guangdong, CN) ; ZHA; Zhengjiong; (Guangdong,
CN) ; WANG; Yongcheng; (Guangdong, CN) |
|
Applicant: |
Name |
City |
State |
Country |
Type |
GUANGZHOU COSMO ENVIRONMENTAL TECHNOLOGY CO., LTD. |
Guangdong |
|
CN |
|
|
Assignee: |
GUANGZHOU COSMO ENVIRONMENTAL
TECHNOLOGY CO., LTD.
Guangdong
CN
|
Family ID: |
1000005100669 |
Appl. No.: |
16/767587 |
Filed: |
December 4, 2017 |
PCT Filed: |
December 4, 2017 |
PCT NO: |
PCT/CN2017/114481 |
371 Date: |
May 27, 2020 |
Current U.S.
Class: |
1/1 |
Current CPC
Class: |
C01P 2004/32 20130101;
C01P 2004/03 20130101; C01P 2004/51 20130101; C01P 2004/61
20130101; C01G 9/04 20130101; A23K 20/30 20160501 |
International
Class: |
C01G 9/04 20060101
C01G009/04; A23K 20/20 20060101 A23K020/20 |
Foreign Application Data
Date |
Code |
Application Number |
Dec 1, 2017 |
CN |
201711252121.5 |
Claims
1. A basic zinc chloride particulate matter, wherein the basic zinc
chloride particulate matter mainly consists of basic zinc chloride
particles; the basic zinc chloride particulate matter has a
D.sub.10 of more than 100 .mu.m and a D.sub.95 of more than 450
.mu.m; the basic zinc chloride particles are free of adhesives;
most of the basic zinc chloride particles contained in the basic
zinc chloride particulate matter have a sphere-like appearance, and
the basic zinc chloride particles having a particle size of more
than 500 .mu.m in the basic zinc chloride particulate matter
account for 1% or less of a total mass of the basic zinc chloride
particulate matter.
2. The basic zinc chloride particulate matter according to claim 1,
wherein the basic zinc chloride particulate matter has a particle
size distribution range of 1 .mu.m to 1000 .mu.m.
3. The basic zinc chloride particulate matter according to claim 1,
wherein the particles having the sphere-like appearance in the
basic zinc chloride particulate matter account for 95% or more of
the total mass of the particulate matter.
4. A preparation method for the basic zinc chloride particulate
matter according to claim 1, wherein the preparation method
comprises the following steps: step S1, preparing a zinc chloride
solution having a zinc concentration of 60 g/L to 150 g/L; step S2,
preparing an ammonia solution having a pH of 10 or more, adding
ammonium chloride as an inducer into the ammonia solution to
prepare a mixed solution, with the ammonium chloride serving as a
main source of chloride ions in the mixed solution, so that the
mixed solution has an ammonia-nitrogen concentration of 140 g/L to
170 g/L and a chloride ion concentration of 80 g/L to 160 g/L; step
S3, complexing and ammonia-leaching of a zinc-containing raw
material by using a mixed solution obtained in step S2 to prepare a
zinc-ammonia complex solution, with a zinc concentration in the
zinc-ammonia complex solution being 60 g/L to 150 g/L; and step S4,
adding water or a mother solution of the basic zinc chloride into a
reaction vessel, heating to 70.degree. C. to 90.degree. C., and
adding the zinc chloride solution in step S1 and the zinc-ammonia
complex solution in step S3 simultaneously in a parallel feeding
manner, maintaining a reaction pH value at 6.0 to 7.0, with a
stirring speed of 1200 r/min to 1500 r/min, and reacting for 2 to 4
hours to obtain a precipitate and a zinc-containing mother
solution, and washing and drying the precipitate to obtain the
basic zinc chloride particulate matter.
5. The preparation method for the basic zinc chloride particulate
matter according to claim 4, wherein the preparation method further
comprises a step of sieving the dried precipitate after completing
step S4 to remove the particles having relatively large particle
size.
6. The preparation method for the basic zinc chloride particulate
matter according to claim 4, wherein the zinc-containing mother
solution in step S4 is subjected to alkali stripping and spraying
absorption to recycle ammonia water.
7. The preparation method for the basic zinc chloride particulate
matter according to claim 4, wherein after removing the
ammonia-nitrogen by alkali stripping, the zinc-containing mother
solution in step S4 is subjected to depth removal of heavy metals,
concentration and crystallization to recycle sodium chloride.
8. The preparation method for the basic zinc chloride particulate
matter according to claim 4, wherein the zinc chloride solution in
step S1 is prepared by the following method: using a
zinc-containing flue dust as a raw material, leaching with acid,
and removing impurities to obtain the zinc chloride solution.
9. The preparation method for the basic zinc chloride particulate
matter according to claim 4, wherein the zinc-containing raw
material is a zinc-containing flue dust, and when using the
zinc-containing flue dust as the raw material, the obtained
zinc-ammonia complex solution is further subjected to a step of
adding zinc powder for replacement and removal of impurities.
10. A feed additive, wherein the feed additive comprises the basic
zinc chloride particulate matter according to claim 1.
11. The basic zinc chloride particulate matter according to claim
2, wherein the particles having the sphere-like appearance in the
basic zinc chloride particulate matter account for 95% or more of
the total mass of the particulate matter.
12. The preparation method for the basic zinc chloride particulate
matter according to claim 5, wherein the zinc-containing mother
solution in step S4 is subjected to alkali stripping and spraying
absorption to recycle ammonia water.
13. The preparation method for the basic zinc chloride particulate
matter according to claim 5, wherein after removing the
ammonia-nitrogen by alkali stripping, the zinc-containing mother
solution in step S4 is subjected to depth removal of heavy metals,
concentration and crystallization to recycle sodium chloride.
14. The preparation method for the basic zinc chloride particulate
matter according to claim 5, wherein the zinc chloride solution in
step S1 is prepared by the following method: using a
zinc-containing flue dust as a raw material, leaching with acid,
and removing impurities to obtain the zinc chloride solution.
15. The preparation method for the basic zinc chloride particulate
matter according to claim 5, wherein the zinc-containing raw
material is a zinc-containing flue dust, and when using the
zinc-containing flue dust as the raw material, the obtained
zinc-ammonia complex solution is further subjected to a step of
adding zinc powder for replacement and removal of impurities.
16. A feed additive, wherein the feed additive comprises the basic
zinc chloride particulate matter according to claim 2.
17. A feed additive, wherein the feed additive comprises the basic
zinc chloride particulate matter according to claim 3.
18. A feed additive, wherein the feed additive comprises the basic
zinc chloride particulate matter according to claim 11.
Description
BACKGROUND
Technical Field
[0001] The present disclosure relates to the field of mineral feed
additives, and specifically relates to a basic zinc chloride
particulate matter and a preparation method therefor.
Description of Related Art
[0002] As a new-type mineral feed additive, and compared with the
conventional mineral feed additives such as zinc sulfate and zinc
oxide, basic zinc chloride possesses advantages of stable chemical
structure, low dosage, high bioavailability and non-agglomeration,
etc. The basic zinc chloride can be synthesized by numerous
existing liquid-solid phase synthesis and liquid-liquid phase
synthesis, but generally the following problems exist: raw
materials are relatively expensive, the synthesized basic zinc
chloride has a small size, large specific surface area, and poor
filtration and washing performances, and becomes powder product
after drying, resulting in a large amount of fugitive dust which
makes the production environment adverse, and most of them are
intermittent reaction production.
[0003] Increasing the particle size of the basic zinc chloride can
effectively solve the problem of fugitive dust, and the prior art
has been making effort to synthesize basic zinc chloride in large
particles. For example, basic zinc chloride powder is subjected to
re-granulation by using an adhesive to increase the particle size
of the basic zinc chloride; or basic zinc chloride particles with
relatively large particle size are synthesized in an organic acidic
induced system, but the addition of organic inducer can increase
difficulties of the subsequent wastewater treatment, and meanwhile,
the basic zinc chloride particles prepared by such method has an
irregular appearance, without good flowability.
[0004] Therefore, it is of great economic value and significance to
develop a mineral feed additive, which is basic zinc chloride, with
no fugitive dust, low production cost and no discharge of waste
water, which can well solve the problems of large amount of
fugitive dust in the working environment and difficulty of
uniformly mixing a premix that exist in process of preparing the
premix by using the basic zinc chloride by the existing feed
enterprises.
SUMMARY
[0005] An objective of the present disclosure is to overcome the
above-mentioned deficiencies of the prior art, and to provide a
basic zinc chloride particulate matter. Basic zinc chloride
particles that constitute the basic zinc chloride particulate
matter has a relatively large particle size and good flowability,
which can satisfy the requirements of no fugitive dust and easy
flowing during the use process in the feed factory.
[0006] Another objective of the present disclosure is to provide a
preparation method for the basic zinc chloride particulate
matter.
[0007] The above objectives of the present disclosure are achieved
by the following technical solutions.
[0008] A basic zinc chloride particulate matter mainly consists of
basic zinc chloride particles. The basic zinc chloride particulate
matter has a D.sub.10 of more than 100 .mu.m and a D.sub.95 of more
than 450 .mu.m. The basic zinc chloride particles are free of
adhesives. Most of the basic zinc chloride particles contained in
the basic zinc chloride particulate matter have a sphere-like
appearance. The basic zinc chloride particles having a particle
size of more than 500 .mu.m in the basic zinc chloride particulate
matter account for 1% or less of a total weight of the basic zinc
chloride particulate matter.
[0009] Fugitive dust is easily caused by the existing basic zinc
chloride, mainly for the reason that the size of the basic zinc
chloride obtained by the conventional methods is too small. Basic
zinc chloride particles with large size can be obtained by the
method of twice granulation or organic inducer, but the process
becomes more complicated, and it is difficult to control the effect
and brings more inconvenience to the post-treatment. Moreover,
addition of an adhesive results in decreased absolute content of
zinc chloride. The basic zinc chloride particulate matter provided
by the present disclosure is prepared by the provided method,
wherein the basic zinc chloride has far larger size which is
uniform simultaneously, and has excellent flowability, compared to
those prepared by any existing methods.
[0010] In the basic zinc chloride particulate matter of the present
disclosure, a content of the basic zinc chloride is 98% or
more.
[0011] Preferably, the particles having a sphere-like appearance
account for 95% or more of the total weight of the particulate
matter, more preferably, 98% or more. The basic zinc chloride
particulate matter having the above-mentioned features of the
present disclosure has an angle of repose of 30.degree. to
35.degree..
[0012] The basic zinc chloride particulate matter of the present
disclosure generally has a particle size distribution range of 1
.mu.m to 1000 .mu.m. The particle size distribution varies within
such range with the process conditions, that is, the minimum size
of the particle size distribution may be more than 1 .mu.m, while
the maximum size of the particle size distribution may be less than
1000 .mu.m. Therefore, if D.sub.10 and D.sub.95 of the products
conform to the above-mentioned range, basic zinc chloride
particulate matter with narrower particle size distribution can be
obtained by the adjustment within the range of 1 .mu.m to 1000
.mu.m.
[0013] For example, in the present disclosure, basic zinc chloride
product with narrower particle size distribution can also be
obtained by manners such as sieving, etc. Preferably, a basic zinc
chloride particulate matter mainly consists of basic zinc chloride
particles. The basic zinc chloride particles in the basic zinc
chloride particulate matter has a particle size distribution of 1
.mu.m to 500 .mu.m, and the basic zinc chloride particulate matter
has a D.sub.10 of more than 100 .mu.m and a D.sub.95 of more than
450 .mu.m. The basic zinc chloride particles are free of adhesives.
Most of the basic zinc chloride particles contained in the basic
zinc chloride particulate matter have a sphere-like appearance.
[0014] The basic zinc chloride particles of the present disclosure
are directly obtained by preparation of the basic zinc chloride,
and thus the basic zinc chloride particles are free of
adhesives.
[0015] A preparation method for the basic zinc chloride particulate
matter, includes the following steps:
[0016] S1, preparing a zinc chloride solution having a zinc
concentration of 60 g/L to 150 g/L;
[0017] S2, preparing an ammonia solution having a pH of 10 or more,
adding ammonium chloride as an inducer into the ammonia solution,
with the ammonium chloride serving as a main source of chloride
ions in the solution, so that a final solution has an
ammonia-nitrogen concentration of 140 g/L to 170 g/L and a chloride
ion concentration of 80 g/L to 160 g/L;
[0018] S3, complexing and ammonia-leaching of a zinc-containing raw
material by using the mixed solution obtained in S2 to prepare a
zinc-ammonia complex solution, with a zinc concentration in the
zinc-ammonia complex solution being 60 g/L to 150 g/L; and
[0019] S4, adding water or a mother solution of the basic zinc
chloride into a reaction vessel, heating to 70.degree. C. to
90.degree. C., and adding the zinc chloride solution in S1 and the
zinc-ammonia complex solution in S3 simultaneously in a parallel
feeding manner, maintaining a reaction pH value at 6.0 to 7.0, with
a stirring speed of 1200 r/min to 1500 r/min, and reacting for 2 to
4 hours to obtain a precipitate and a zinc-containing mother
solution, and washing and drying the precipitate to obtain the
basic zinc chloride particulate matter.
[0020] It can be observed and found by scanning electron microscope
that appearance of most of the basic zinc chloride particles
prepared by the method of the present disclosure is nearly
sphere-like, thus having better flowability. By using ammonium
chloride as an inducer, no impurities are introduced additionally,
so that wastewater treatment is simple. By controlling the
parameters such as the reaction pH value and stirring speed, the
basic zinc chloride product which is sphere-like and has large
particle size is prepared, and the product has advantages of
no-fugitive dust, good flowability, etc.
[0021] In order to obtain the basic zinc chloride particulate
matter with narrower particle size distribution of the present
disclosure, preferably the preparation method further comprises a
step of sieving the dried precipitate after completing S4 to remove
the particles having relatively large particle size. Through
sorting by a sieving device, the basic zinc chloride particulate
matter with narrower particle size distribution range can be
obtained.
[0022] Preferably, the sieving is to collect a particulate matter
which can pass through a 35-mesh sieve.
[0023] Preferably, the zinc-containing mother solution in S4 is
subjected to alkali stripping and spraying absorption to recycle
ammonia water.
[0024] Preferably, after removing the ammonia-nitrogen from the by
alkali stripping, the zinc-containing mother solution in S4 is
subjected to depth removal of heavy metals, concentration and
crystallization to recycle sodium chloride.
[0025] Preferably, the zinc chloride solution in S1 is prepared by
the following method: using a zinc-containing flue dust as a raw
material, leaching with acid, and removing impurities to obtain the
zinc chloride solution. The flue dust is production waste of steel
plants, and using the flue dust to prepare zinc chloride solution
can realize the utilization of waste products which is economic and
environmental.
[0026] Preferably, the zinc-containing raw material is a
zinc-containing flue dust, and when using the zinc-containing flue
dust as the raw material, the obtained zinc-ammonia complex
solution is further subjected to a step of adding zinc powder for
replacement and removal of impurities.
[0027] A feed additive includes the basic zinc chloride particulate
matter.
[0028] The zinc chloride solution in S1 can also be obtained by
dissolving a zinc chloride solid or a zinc oxide solid into water
or hydrochloric acid solution.
[0029] Main components of the wastewater which is generated during
preparation of the basic zinc chloride by the present method is
zinc-ammonia complex and ammonium chloride.
[0030] Ammonia, zinc hydroxide and distilled water can be recycled
by simply processing the wastewater, guaranteeing a closed cycle of
zinc and ammonia-nitrogen, without discharge of wastewater during
the whole technological process, and realizing a continuously
environmental production.
[0031] Compared with the prior art, the present disclosure has the
following beneficial effects.
[0032] The present disclosure provides a basic zinc chloride
particulate matter and a preparation method therefor. The basic
zinc chloride particulate matter has relatively large particle size
and good flowability, which is easy to flow without fugitive dust
when in use, solving the problems of large amount of fugitive dust
in the working environment and difficulty of uniformly mixing a
premix that exist in process of preparing the premix by using the
basic zinc chloride by the existing feed enterprises. The
preparation process of the present disclosure uses ammonium
chloride as an inducer, no impurities are introduced additionally,
and the production of wastewater can be recycled completely, with
low production cost and environmental and economic production
process.
BRIEF DESCRIPTION OF THE DRAWINGS
[0033] FIG. 1 is a particle size distribution diagram of a basic
zinc chloride particulate matter prepared in Embodiment 1.
[0034] FIG. 2 is a SEM diagram of magnification of 300 times the
basic zinc chloride particulate matter prepared in Embodiment
1.
[0035] FIG. 3 is a SEM diagram of magnification of 100 times the
basic zinc chloride particulate matter prepared in Embodiment
1.
[0036] FIG. 4 is a SEM diagram of magnification of 50 times the
basic zinc chloride particulate matter prepared in Embodiment
1.
[0037] FIG. 5 is a SEM diagram of magnification of 30 times the
basic zinc chloride particulate matter prepared in Embodiment
1.
[0038] FIG. 6 is a particle size distribution diagram of a
commercially available basic zinc chloride product.
[0039] FIG. 7 is a SEM diagram of magnification of 300 times the
commercially available basic zinc chloride product.
[0040] FIG. 8 is a SEM diagram of magnification of 100 times the
commercially available basic zinc chloride product.
[0041] FIG. 9 is a SEM diagram of magnification of 50 times the
commercially available basic zinc chloride product.
[0042] FIG. 10 is a SEM diagram of magnification of 30 times the
commercially available basic zinc chloride product.
DESCRIPTION OF THE EMBODIMENTS
[0043] The present disclosure is further described below in
combination with specific implementations, but the present
disclosure is not limited by the embodiments in any ways.
[0044] Unless otherwise, raw materials and reagents used in the
embodiments of the present disclosure are conventional raw
materials and reagents which are commercially available.
[0045] Commercially available basic zinc chloride was purchased
from the commercially available product which conforms to Chinese
standard Feed Additive--Basic Zinc Chloride (GB/T 22546-2008).
[0046] Test method of angle of repose was performed according to
Surface active agents--Powders and granules--Measurement of the
angle of repose (GB/T 11986-1898).
[0047] Particle size distribution, D.sub.10 and D.sub.95 were
determined by using GB/T19077-2016 Laser Diffraction Methods.
[0048] Morphology of the basic zinc chloride was observed by a
scanning electron microscope.
EMBODIMENTS
[0049] S1, zinc oxide was dissolved in a hydrochloric acid solution
to prepare a zinc chloride solution;
[0050] S2, an ammonia solution having a pH of 10 or more was
prepared, ammonium chloride was added as an inducer into the
ammonia solution, the ammonium chloride served as a main source of
chloride ions in the solution so that a final solution had an
ammonia-nitrogen concentration of 140 g/L to 170 g/L and a chloride
ion concentration of 80 g/L to 160 g/L;
[0051] S3, zinc oxide was subjected to complexing and
ammonia-leaching by using a mixed solution obtained in S2 to
prepare a zinc-ammonia complex solution; and
[0052] S4, water was added into a reaction vessel, followed by
heating to 70.degree. C. to 90.degree. C., and the zinc chloride
solution in S1 and the zinc-ammonia complex solution in S3 were
simultaneously added in a parallel feeding manner, a reaction pH
value was maintained at 6.0 to 7.0, and the reaction lasted for 2
to 4 hours to obtain a precipitate and a zinc-containing mother
solution; and a basic zinc chloride particulate matter in beige or
white was obtained by washing and drying the precipitate.
[0053] Specific parameters of each embodiment are shown in Table
1.
TABLE-US-00001 TABLE 1 S1, zinc S2, S3, zinc content ammonia- S2,
content in in the nitrogen chloride the zinc content in content in
zinc-ammonia chloride the final the final complex S4, stirring
solution solution solution solution speed Reaction (g/L) (g/L)
(g/L) (g/L) (r/min) duration Embodiment 1 60 140 80 60 1200 2
Embodiment 2 150 140 80 60 1200 2 Embodiment 3 60 170 80 110 1200 2
Embodiment 4 60 140 80 60 1500 2 Embodiment 5 110 155 80 110 1300 4
Embodiment 6 110 155 160 110 1300 4 Embodiment 7 110 155 120 110
1300 4
Embodiment 8
[0054] S1, a zinc-containing flue dust was used as a raw material,
by leaching with acid, and removing impurities, a zinc chloride
solution was obtained; water was added to the solution to adjust a
zinc concentration to 60 g/L, and a purified zinc chloride solution
was obtained;
[0055] S2, an ammonia solution having a pH of 10 or more was
prepared, ammonium chloride was added as an inducer into the
ammonia solution, the ammonium chloride served as a main source of
chloride ions in the solution so that a final solution had an
ammonia-nitrogen concentration of 140 g/L to 170 g/L and a chloride
ion concentration of 80 g/L to 160 g/L;
[0056] S3, the zinc-containing flue dust was added to a mixed
solution prepared in S2 for complexing and ammonia-leaching, when a
zinc concentration in the liquid phase reached to 60 g/L, filtering
separation was performed, ammonia-leaching of the solid phase was
continued, zinc powder was added to the liquid phase for
replacement and removal of impurities, and a purified zinc-ammonia
complex solution was obtained;
[0057] S4, synthesis of basic zinc chloride
[0058] water was added into a reaction vessel, followed by heating
to 70.degree. C., and the purified zinc chloride solution and the
zinc-ammonia complex solution were simultaneously added in a
parallel feeding manner, a reaction pH value was maintained at 6.0
to 7.0, and the reaction lasted for 2 hours to obtain a precipitate
and a zinc-containing mother solution; and a basic zinc chloride
particulate matter was obtained by washing and drying the
precipitate; and
[0059] S5, wastewater treatment
[0060] sodium hydroxide was added to the zinc-containing mother
solution for steam stripping, and gaseous phase was subjected to
spraying absorption to recycle ammonia water which can be reused in
the production or for sale; solid phase obtained by ammonia
distillation of liquid phase was the zinc hydroxide solid which can
be returned to the front end and dissolved in the hydrochloric acid
to prepare the zinc chloride solution for reuse in the production;
after the wastewater rid of ammonia-nitrogen was subjected to depth
removal of heavy metals, sodium chloride can be recycled by MVR
concentration and crystallization, and the evaporated moisture can
be reused in production as recycled water after cooling, without
discharge of wastewater.
Comparative Example 1
[0061] Basically the same as the above-mentioned Embodiment 1, but
a reaction pH value in the synthesis of the basic zinc chloride in
S4 was set as 5.
Comparative Example 2
[0062] Basically the same as the above-mentioned Embodiment 1, but
a reaction pH value in the synthesis of the basic zinc chloride in
S4 was set as 8.
Comparative Example 3
[0063] Basically the same as the above-mentioned Embodiment 1, but
a stirring speed in the synthesis of the basic zinc chloride in S4
was set as 1600 r/min.
Comparative Example 4
[0064] Basically the same as the above-mentioned Embodiment 1, but
a stirring speed in the synthesis of the basic zinc chloride in S4
was set as 1100 r/min.
Comparative Example 5
[0065] Basically the same as the above-mentioned Embodiment 6, but
a chloride ion concentration in the mixed solution obtained in S2
was 70 g/L.
Comparative Example 6
[0066] Basically the same as the above-mentioned Embodiment 6, but
a chloride ion concentration in the mixed solution obtained in S2
was 170 g/L.
[0067] The basic zinc chloride particulate matters prepared by each
of the embodiments and comparative examples were subjected to the
particle size distribution test and flowability test, and the
results are as shown in Table 2.
TABLE-US-00002 TABLE 2 Angle of Particle repose of basic size range
zinc chloride Basic zinc of basic zinc particulate chloride content
chloride D.sub.10 D.sub.95 matter in particulate (.mu.m) (.mu.m)
(.mu.m) (degree) Morphology matter (%) Embodiment 1 4~900 106 518
30 Sphere-like 98.5 white particles Embodiment 2 10~880 115 530 32
Sphere-like 98.6 white particles Embodiment 3 8~850 112 550 35
Sphere-like 98.6 white particles Embodiment 4 5~890 118 515 33
Sphere-like 98.6 white particles Embodiment 5 10~810 115 540 35
Sphere-like 98.7 white particles Embodiment 6 15~750 120 579 35
Sphere-like 98.8 white particles Embodiment 7 15~690 118 575 35
Sphere-like 98.8 white particles Embodiment 8 6~800 108 560 31
Sphere-like 98.7 white particles Comparative 1~80 45 78 58 White
96.7 Example 1 powder Comparative 1~90 55 85 65 White 97.5 Example
2 powder Comparative 1~105 62 100 55 White 96.1 Example 3 powder
Comparative 1~300 83 288 48 White solid 97.5 Example 4 Comparative
1~120 44 115 52 White 96.2 Example 5 powder Comparative 1~180 52
160 50 White 97.1 Example 6 powder Commercially 1~110 20 100 55~60
Beige 98.1 available basic powder zinc chloride particulate
matter
[0068] It can be seen from the data of the above-mentioned
embodiments and comparative examples that the pH value, the
chloride ion content in the ammonia solution and the stirring speed
exert a significant effect on the prepared basic zinc chloride
particles. The basic zinc chloride particles prepared within the pH
value range of the present disclosure have a sphere-like shape, an
angle of repose of 30.degree. to 35.degree., and excellent
flowability, which are conducive to storage and uniform mixing of
the premix. The basic zinc chloride particles have a D.sub.10 of
more than 100 .mu.m and a D.sub.95 of more than 450 .mu.m,
indicating that most of them are particles with relatively large
particle size, and the particle size is uniform. They are more
convenient in use, compared with the commercially available basic
zinc chloride product of which the particle size is too small and
uneven. It can be seen from the comparative examples that particles
with large particle size may also be obtained (for example,
Comparative Example 4) even though the preparation process is out
of the scope of the present disclosure, but such product still has
bad flowability performance and is difficult to be dispersed.
[0069] The basic zinc chloride particulate matters prepared by
Embodiments 1 to 8 were sieved through a 35-mesh sieve, particles
which can pass through the 35-mesh sieve were collected, and
D.sub.10 and D.sub.95 thereof were measured. Results are as shown
in Table 3.
TABLE-US-00003 TABLE 3 Particle size Angle of range of repose of
Basic zinc basic zinc basic zinc chloride Weight Weight chloride
chloride content in before after after particulate particulate
sieving sieving sieving D.sub.10 D.sub.95 matter matter (g) (g)
(.mu.m) (.mu.m) (.mu.m) (degree) Morphology (%) Embodiment 1 200
198.9 4~450 115 488 30 Sphere-like 98.8 white particles Embodiment
2 200 199.3 10~450 115 510 30 Sphere-like 98.6 white particles
Embodiment 3 200 199.4 8~450 110 550 35 Sphere-like 98.6 white
particles Embodiment 4 200 199.1 5~450 120 485 30 Sphere-like 98.6
white particles Embodiment 5 200 198.4 10~450 125 510 35
Sphere-like 98.7 white particles Embodiment 6 200 198.8 15~450 110
479 35 Sphere-like 98.1 white particles Embodiment 7 200 198.7
15~450 108 475 35 Sphere-like 98.2 white particles Embodiment 8 200
198.5 6~450 117 480 35 Sphere-like 98.7 white particles
* * * * *